تفاعل #90252

ord-cec6d26d3d2a41c4af2ff2d5cd988d37

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىSolvent was evaporated
  2. 2
    workup.ADDITIONthe residue was treated with 1 N HCl (50 mL)
  3. 3
    workup.STIRRINGstirred for 10 minutes
  4. 4
    ترشيحYellow product was collected by filtration
  5. 5
    غسيلwashed with water and methanol
  6. 6
    أخرىdried
  7. 7
    أخرىCrude material was crystallized from chloroform-ethanol
  8. 8
    أخرىto provide 900 mg (80%) of yellow 11-4

الإجراء التجريبي

To a solution of 10-methyl-9-oxo-9,10-dihydroacridine-2,7-disulfonyl dichloride from Example 7 (810 mg, 2 mmole) in THF (20 mL) was added 3,5-dimethylpiperidine (2 mL, 15 mmole) and the reaction mixture was stirred at room temperature for 6 hours. Solvent was evaporated and the residue was treated with 1 N HCl (50 mL) and stirred for 10 minutes. Yellow product was collected by filtration, washed with water and methanol and dried. Crude material was crystallized from chloroform-ethanol to provide 900 mg (80%) of yellow 11-4. MS 560 (MH+).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09446021B2uspto-grants-2016_09